Method for measuring calcium constituent in silicon aluminum calcium barium alloy

A technology of calcium element and calcium barium, which is applied in the field of analytical chemistry, can solve problems such as slow discoloration reaction, excessive hydrofluoric acid, and environmental pollution, and achieve the effects of reducing operation links, eliminating barium interference, and reducing uncertainty

Inactive Publication Date: 2009-01-14
WUHAN IRON & STEEL (GROUP) CORP
View PDF0 Cites 27 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After analysis, although this method can measure the content of barium and calcium at the same time, its disadvantages are: the first is that the calcium in the solution is not fully released due to the one-time addition of 20 ml of perchloric acid; the second is that the discoloration reaction at the end of the solution is

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for measuring calcium constituent in silicon aluminum calcium barium alloy
  • Method for measuring calcium constituent in silicon aluminum calcium barium alloy
  • Method for measuring calcium constituent in silicon aluminum calcium barium alloy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A method for determining calcium in silicon-aluminum-calcium-barium alloy, and its steps:

[0032] 1) Take the sample (YSB14612 Ca: 9.25%) 0.1000 g sample and place it in a polytetrafluoroethylene beaker, and add deionized water until the sample is wet;

[0033] 2) Add 10 ml of nitric acid;

[0034] 3) Add 1 ml of hydrofluoric acid dropwise;

[0035] 4) Heat on the electric heating plate until the sample is completely dissolved;

[0036] 5) Add 4.5 ml of perchloric acid;

[0037] 6) Heat at 170℃ until the sample volume is reduced to 2 ml;

[0038] 7) Naturally cool to 25℃;

[0039] 8) Add 4.5 ml of perchloric acid and heat at 170°C until the sample volume is reduced to 2 ml;

[0040] 9) Add 10 ml of hydrochloric acid and 50 ml of deionized water;

[0041] 10) Heat at 100°C until the salt is dissolved, take it off and cool the sample to 38°C by natural cooling;

[0042] 11) Put the cooled sample into a 100 ml graduated volumetric flask, dilute to 100 ml graduated with deioni...

Embodiment 2

[0048] A method for determining calcium in silicon-aluminum-calcium-barium alloy, and its steps:

[0049] 1) Take a sample (YSB14612 Ca: 9.25%) 0.2800g sample and place it in a polytetrafluoroethylene beaker, and add deionized water until the sample is wet;

[0050] 2) Add 10 ml of nitric acid;

[0051] 3) Add 1 ml of hydrofluoric acid dropwise;

[0052] 4) Heat on the electric heating plate until the sample is completely dissolved;

[0053] 5) Add 4.5 ml of perchloric acid;

[0054] 6) Heat at 180℃ until the sample volume is reduced to 1.5ml;

[0055] 7) Naturally cool to 25℃;

[0056] 8) Add 4.5 ml of perchloric acid and heat it at 180°C until the sample volume is reduced to 1.5 ml;

[0057] 9) Add 10 ml of hydrochloric acid and 50 ml of deionized water;

[0058] 10) Heat at 100°C until the salt is dissolved, take it off and cool the sample to below 35°C by natural cooling;

[0059] 11) Put the cooled sample into a 100 ml graduated volumetric flask, dilute to 100 ml graduated wi...

Embodiment 3

[0065] A method for determining calcium in silicon-aluminum-calcium-barium alloy, and its steps:

[0066] 1) Take a sample (YSB14612Ca: 9.25%) 0.6 g of the sample and place it in a polytetrafluoroethylene beaker, and add deionized water until the sample is wet;

[0067] 2) Add 10.5 ml of nitric acid;

[0068] 3) Add 1.5 ml of hydrofluoric acid dropwise;

[0069] 4) Heat on the electric heating plate until the sample is completely dissolved;

[0070] 5) Add 5.0 ml of perchloric acid;

[0071] 6) Heat at 185℃ until the sample volume is reduced to 1.3ml;

[0072] 7) Naturally cool to 28℃;

[0073] 8) Add 5.0 ml of perchloric acid and heat at 190℃ until the sample volume is reduced to 1.3 ml;

[0074] 9) Add 9.5 ml of hydrochloric acid and 50 ml of deionized water;

[0075] 10) Heat to complete dissolution at 110°C, remove it, and cool the sample to 30°C by natural cooling;

[0076] 11) Put the cooled sample into a 100 ml graduated volumetric flask, dilute to 100 ml graduated with deion...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a method used for measuring the calcium element in a silicon, aluminum, calcium and barium alloy, which comprises the following steps: a test sample is placed in a beaker, and deionized water is added until the test sample is wet; 9.5 to 10.5 millimeter of nitric acid is added; 1 to 2 millimeter of hydrofluoric acid is titrated; the mixture solution is heated until completely dissolved; perchloric acid is added; the mixture solution is heated until the sample volume is reduced to 1 to 2 millimeter; the mixture solution is naturally cooled; the perchloric acid is further added, and the mixture solution is heated until the sample volume is reduced to 1 to 2 millimeter; the hydrochloric acid and the deionized water are further added; the mixture solution is heated until all salts are dissolved, and the mixture solution is naturally cooled until the temperature is lower than 40 DEG C; the test sample is placed into a volumetric flask with scales and diluted with the deionized water; a mother solution is placed into a trigonal cup, the deionized water, trolamine (1 added by 1), lemery, bitter salt and an calcon-carboxylic acid are added, and the mother solution is adjusted to be red with potassium hydroxide; the potassium hydroxide is further added; EDTA is titrated until an end point that the mother solution becomes blue; and an analyzing result is computed. The method does not need precipitation separation and filtration, and has the acute end point without intermediate color and improved measuring accuracy.

Description

Technical field [0001] The invention relates to the field of analytical chemistry, and belongs to an analytical method for determining calcium in a silicon-aluminum-calcium-barium alloy by adopting an EDTA direct titration method. Background technique [0002] At present, the detection methods of calcium in silicon-aluminum-calcium-barium alloys generally use ammonia to separate iron and aluminum, ammonium persulfate to separate manganese, potassium sulfate to precipitate barium, calcium indicator as indicator, EDTA titration. This method is cumbersome to operate, has a long analysis cycle and high cost. [0003] In order to improve the efficiency of analysis and testing, people have done a lot of work around the element analysis of silicon-aluminum-calcium-barium alloys and have achieved certain results, such as the "Silicon-aluminum-Calcium-Barium Alloy In the article "Determination of Medium Barium and Calcium", it is disclosed that the content of barium and calcium can be mea...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): G01N21/79
Inventor 李洁周正伦谢芬宋建红程运娥刘秀莹张杰
Owner WUHAN IRON & STEEL (GROUP) CORP
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap